高效液相色谱-串联质谱法快速测定甘蔗中杀虫双残留量

Fast Detection of Bisultap Residue in Sugarcane by Liquid Chromatography-Tandem Mass Spectrometry

建立了一种简便、快速、灵敏、准确的甘蔗中杀虫双的液相色谱-串联质谱分析方法。优化了色谱、质谱条件和提取溶剂的组成,以甲醇-水（50∶50,V/V）提取样品中的杀虫双,离心后上层清液过滤后直接上机检测,无需进一步净化。甘蔗中杀虫双的检出限为1.0μg/kg,定量限为4.0μg/kg。甘蔗中5个添加量4.0、10、100、200μg/kg和500μg/kg的回收率为62.3%~108.4%,相对标准偏差为5.1%~14.8%。采用本方法分析了8例广州市场上的甘蔗样品,均未检出杀虫双。

In this study, a simple, fast, sensitive and accurate liquid chromatography-tandem mass spectrometry（LC-MS-MS） method was developed for the analysis of bisultap in sugarcane. The chromatographic conditions, the mass spectrometry parameters and the composition of extraction solvent were optimized. Bisultap was extracted with 50% methanol-water（50：50, V/V）. Then, the extraction phase was filtered after centrifugation, followed by LC-MS-MS detection without further purification. The limit of detection for bisultap in sugarcane was 1.0 μg/kg and the limit of quantification was 4.0 μg/kg. Recoveries at five spiked levels of 4.0, 10, 100, 200 and 500 μg/kg ranged from 62.3% to 108.4% with relative standard deviations of 5.1% to 14.8%. The proposed method was applied to the analysis of eight sugarcane samples from local markets in Guangzhou and no bisultap was detected.